Preparation method of chlorpheniramine maleate impurities
A kind of technology of chlorpheniramine acid and impurity, which is applied in the field of preparation of chlorpheniramine maleate impurity, can solve problems such as shortage of certified products, and achieve the effects of being conducive to quality control, high purity, and simple and feasible process operation.
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Embodiment 1
[0031] The present embodiment provides a kind of preparation method of chlorpheniramine maleate impurity, and the steps are as follows:
[0032] (1) Add compound 1 (2.04g, 10mmol) into 30mL toluene, weigh sodium amide (0.98g, 25mmol) into the above toluene solution, add N-(tert-butoxycarbonyl)-2-chloroethylamine Solid (1.97g, 11mmol) and tetrabutylammonium chloride (140mg, 0.5mmol), react at 65-70°C for 5-6h, add water 10mL after cooling to quench the reaction, extract and separate the liquid, and concentrate the organic phase to remove the solvent , to obtain 3.11 g of compound 2, with a yield of 89.7%.
[0033] (2) Add the compound 2 oil obtained in step (1) into 25mL of toluene, weigh sodium borohydride (750mg, 20mmol) into the above toluene solution, react at 75-85°C for 4-5h, and add 10mL of water after cooling to quench The reaction was quenched, extraction and liquid separation were carried out, and the organic phase was concentrated to remove the solvent to obtain 1.8...
Embodiment 2
[0035] The present embodiment provides a kind of preparation method of chlorpheniramine maleate impurity, and the steps are as follows:
[0036] (1) Add compound 1 (2.04g, 10mmol) into 30mL toluene, weigh sodium amide (0.98g, 25mmol) into the above toluene solution, add N-(tert-butoxycarbonyl)-2-chloroethylamine Solid (1.97g, 11mmol) and tetramethylammonium chloride (55mg, 0.5mmol), react at 65-70°C for 4-5h, add water 10mL after cooling to quench the reaction, extract and separate the liquid, and concentrate the organic phase to remove the solvent , to obtain 3.16g of compound 2, yield 91.3%.
[0037] (2) Add the compound 2 oil obtained in step (1) into 25mL of toluene, weigh lithium tetrahydrogen aluminum (0.72g, 20mmol) into the above toluene solution, react at 75-85°C for 4-5h, add water after cooling 10 mL was used to quench the reaction, extract and separate the liquids, and the organic phase was concentrated to remove the solvent to obtain 2.10 g of the target compound...
Embodiment 3
[0039] The present embodiment provides a kind of preparation method of chlorpheniramine maleate impurity, and the steps are as follows:
[0040] (1) Add compound 1 (2.04g, 10mmol) into 30mL toluene, weigh sodium amide (0.98g, 25mmol) into the above toluene solution, add N-(tert-butoxycarbonyl)-2-chloroethylamine Solid (1.97g, 11mmol) and tetrabutylammonium bromide (0.16g, 0.5mmol), react at 65-70°C for 2-3h, add 10mL of water after cooling to quench the reaction, extract and separate the liquid, and remove the organic phase by concentrating The solvent was used to obtain 3.32 g of compound 2, with a yield of 95.3%.
[0041] (2) Add the compound 2 oil obtained in step (1) into 25mL of toluene, weigh lithium tetrahydrogen aluminum (0.72g, 20mmol) into the above toluene solution, react at 75-85°C for 4-5h, add water after cooling 10 mL was used to quench the reaction, extract and separate the liquids, and the organic phase was concentrated to remove the solvent to obtain 2.25 g ...
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